Method for preparing methyl levulinate through clean conversion of biomass sugar and separating methyl levulinate

A technology of methyl levulinate and biomass sugar, applied in the preparation of organic compounds, separation/purification of carboxylic acid esters, chemical instruments and methods, etc., can solve the problem of increased reaction pressure, reduced methanol recovery, equipment corrosion, etc. problems, to achieve the effects of less side reactions, easy separation, and convenient operation

Inactive Publication Date: 2012-04-04
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of these liquid acid catalysts will cause some problems, such as: serious corrosion of equipment, need to use expensive high-nickel alloy reactor; easy dehydration between methanol molecules to form methyl ether, because the boiling point of methyl ether is very low (-24.9 ℃) It leads to a significant increase in the reaction pressure, and also reduces the amount of methanol recovered; the waste acid after the reaction needs to be neutralized, resulting in a large amount of waste liquid and waste residue

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a 100 mL autoclave, add 2.5 g of glucose and SO at 550 °C for 3 h 4 2– / TiO 2 Catalyst 1.25 g and anhydrous methanol 50 mL; after sealing the reactor, heat up to 200 °C for 2 h at a stirring speed of 500 r / min; after the reaction, cool the reactor to room temperature, take out the sample, and filter to separate the liquid product and solid matter; the liquid product was first distilled at 80 °C to remove low-boiling substances; after the distillation, 5 mL of n-dodecane was added to the residue as a steaming aid, and rotary distillation was performed under reduced pressure at 160 °C, and the distillate was collected. The liquid is discharged; the distillate is automatically stratified and analyzed by gas chromatography mass spectrometry. The upper layer is n-dodecane, which can be reused; the lower layer is methyl levulinate, with a mass of 0.45 g and a molar yield of 24.8%.

Embodiment 2

[0032] In a 100 mL autoclave, add 2.5 g of glucose and SO at 450 °C for 3 h 4 2– / TiO 2 Catalyst 1.25 g and anhydrous methanol 50 mL; after sealing the reactor, heat up to 200 °C for 2 h at a stirring speed of 500 r / min; after the reaction, cool the reactor to room temperature, take out the sample, and filter to separate the liquid product and solid matter; the liquid product was first distilled at 80 °C to remove low-boiling substances; after the distillation, 5 mL of n-dodecane was added to the residue as a steaming aid, and rotary distillation was performed under reduced pressure at 160 °C, and the distillate was collected. The liquid is discharged; the distillate is automatically stratified and analyzed by gas chromatography mass spectrometry. The upper layer is n-dodecane, which can be reused; the lower layer is methyl levulinate, with a mass of 0.80 g and a molar yield of 44.6%.

[0033] After the solid was calcined at 450 °C for 3 h, the recovered SO 4 2– / TiO 2 Th...

Embodiment 3

[0035] In a 100 mL autoclave, add 2.5 g of glucose and SO at 450 °C for 3 h 4 2– / ZrO 2 Catalyst 1.25 g and anhydrous methanol 50 mL; after sealing the reactor, heat up to 200 °C for 2 h at a stirring speed of 500 r / min; after the reaction, cool the reactor to room temperature, take out the sample, and filter to separate the liquid product and solid matter; the liquid product was first distilled at 80 °C to remove low-boiling substances; after the distillation, 5 mL of n-dodecane was added to the residue as a steaming aid, and rotary distillation was performed under reduced pressure at 160 °C, and the distillate was collected. The liquid is discharged; the distillate is automatically stratified and analyzed by gas chromatography mass spectrometry. The upper layer is n-dodecane, which can be reused; the lower layer is methyl levulinate, with a mass of 0.66 g and a molar yield of 36.8%.

[0036] After the solid was calcined at 450 °C for 3 h, the recovered SO 4 2– / ZrO 2The...

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PUM

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Abstract

The invention discloses a method for preparing methyl levulinate through the clean conversion of biomass sugar and separating methyl levulinate. The method comprises the following steps: 1, calcinating a solid acid at 300-700DEG C for 1-5h; 2, adding a biomass sugar methanol solution with the mass concentration of 10-200g/L and the solid acid to a high pressure reactor to obtain a mixed solution; 3, heating the mixed solution to 180-220DEG C, and keeping the temperature for 1-5h; 4, cooling to room temperature, and separating a solid catalyst from a liquid product by filtering; 5, carrying out normal pressure distillation on the liquid product to remove low boiling point substances to obtain a residue; and 6, adding a distillation assistant to the residue, and carrying out reduced pressure distillation to obtain methyl levulinate. The method of the invention, which adopts the clean solid super acid to catalyze the conversion of the biomass sugar into methyl levulinate and has the advantages of no corrosion to equipment, easy separation of the catalyst from the product, environment protection and the like, accords with the greening development trend of the current chemical industry.

Description

technical field [0001] The present invention relates to a method for the preparation and separation of esters, in particular to a method for cleanly transforming biomass sugar to prepare methyl levulinate and its separation. The method uses a solid acid catalyst to cleanly transform under mild near-critical conditions Preparation of methyl levulinate from biomass sugar and addition of steaming aid to distill and separate the product. Background technique [0002] Methyl levulinate (Methyl Levulinate, CAS No: 624-45-3), also known as methyl pentanoate, methyl 4-oxopentanoate or methyl 4-oxopentanoate, it is levulinate A class of organic compounds produced after methanol esterification. [0003] At present, most industries use levulinic acid to directly esterify methyl levulinate under acidic conditions with methanol to prepare methyl levulinate. The raw material levulinic acid used in this method is relatively expensive, resulting in higher production costs of methyl levulin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/00C07C67/48
Inventor 庄军平林鹿彭林才庞春生
Owner SOUTH CHINA UNIV OF TECH
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